Sabzevari O, Abdi Kh, Amini M, Shafiee A
Department of Toxicology and Pharmacology, Faculty of Pharmacy, Tehran University of Medical Sciences, Tehran, Iran.
Anal Bioanal Chem. 2004 May;379(1):120-4. doi: 10.1007/s00216-004-2563-8. Epub 2004 Mar 13.
Thirty hair samples were collected from male opioid abusers for whom the presence of morphine in their urine samples was confirmed by thin layer chromatography (TLC). The hair samples were decontaminated by washing with isopropanol, deionized water, and isopropanol, dried at room temperature, and cut into small pieces. Samples of the latter (30 mg ) were digested by incubation in a mixture of methanol-trifluoroacetic acid (9:1) for 18 h at 45 degrees C and sonicated to improve the extraction process. The methanolic phase was evaporated to dryness under a stream of nitrogen at 50 degrees C. The sample was derivatized by addition of N-methyl- N-trimethylsilyltrifluoroacetamide (MSTFA) and 1% trimethyliodosilane (TMIS) at 70 degrees C for 20 min, with sonication. Derivatized samples (1 microL) were injected into a gas chromatograph-mass spectrometer (GC-MS) system fitted with a capillary column; the Finnigan MS was operated in SIM mode. Naltrexone was used as internal standard (IS). The masses of the ions selected for morphine and naltrexone were 429 and 557, respectively. The limit of quantitation was set at 0.03 ng mg(-1) hair. By using the above procedure we detected morphine in all the samples examined, in the concentration range 0.26-10.31 ng mg(-1 )hair.
从男性阿片类药物滥用者身上采集了30份毛发样本,这些人的尿液样本中吗啡的存在已通过薄层色谱法(TLC)得到证实。毛发样本先用异丙醇、去离子水和异丙醇洗涤进行去污处理,在室温下干燥,然后切成小块。将后者的样本(30毫克)在甲醇 - 三氟乙酸(9:1)的混合物中于45℃孵育18小时进行消化,并进行超声处理以改善提取过程。在50℃的氮气流下将甲醇相蒸发至干。通过在70℃加入N - 甲基 - N - 三甲基硅烷基三氟乙酰胺(MSTFA)和1%三甲基碘硅烷(TMIS)并超声处理20分钟对样本进行衍生化。将衍生化后的样本(1微升)注入配备毛细管柱的气相色谱 - 质谱联用仪(GC - MS)系统;Finnigan MS以选择离子监测(SIM)模式运行。纳曲酮用作内标(IS)。为吗啡和纳曲酮选择的离子质量分别为429和557。定量限设定为0.03纳克/毫克(-1)毛发。通过使用上述程序,我们在所检测的所有样本中都检测到了吗啡,其浓度范围为0.26 - 10.31纳克/毫克(-1)毛发。